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Antiperspirant Active Compositions and Manufacture Thereof

a technology of active compositions and antiperspirants, applied in the field of antiperspirant active compositions, can solve the problems of reducing antiperspirant efficacy and unacceptably low alsub>, and achieve the effects of high antiperspirant efficacy, high antiperspirant efficacy, and high antiperspirant efficacy

Inactive Publication Date: 2013-08-15
COLGATE PALMOLIVE CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

The present invention is about a new method for producing an effective and stable antiperspirant active ingredient that contains a high amount of Al30 polyhydroxyoxoaluminum cation. This ingredient has a high antiperspirant efficacy but low Peak 3 area, which reduces the amount of other large aluminum species that can also elute under SEC Peak 3. The method involves heating an aqueous solution of an aluminum salt containing a specific ratio of aluminum to chloride, buffer, OH:Al, and pH. This heating process forms a stable and effective antiperspirant active ingredient with high antiperspirant efficacy.

Problems solved by technology

Therefore the data published by Chen et al shows that prolonged heating of an Al13 solution with the aim of trying to synthesize Al30 may result in unacceptably low Al30 concentrations and, importantly for aluminum antiperspirant actives, produce NMR-inactive Al species that may elute under Peak 2 or Peak 3 and reduce antiperspirant efficacy.

Method used

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  • Antiperspirant Active Compositions and Manufacture Thereof
  • Antiperspirant Active Compositions and Manufacture Thereof
  • Antiperspirant Active Compositions and Manufacture Thereof

Examples

Experimental program
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example 1

[0185]An aqueous solution of 0.5M AlCl3.6H2O (50 mmol) was buffered with 1.23M glycine (123 mmol) and heated to 95° C. under vigorous stirring. To this solution, a 1 N Ca(OH)2 (61.5 mmol) was added dropwise over a 2 hour 30 minute period until a final molar ratio of OH:Al of 2.46 was achieved. The pH after the reaction was 3.8. A 50 ml aliquot was removed and subjected to testing by SEC chromatography and 27Al NMR spectroscopy.

[0186]In this specification, the use of 27Al NMR data is not quantitative but considers only NMR-visible Al species and in particular resonances at 0 ppm, 62.5 ppm and 70 ppm. When calculating the relative amounts of Al embodied in the Al13 and Al30 polyhydroxyoxoaluminum cations, the tetrahedral resonance peak is integrated and must be multiplied by a scaling factor to account for other octahedrally coordinated Al present in the structure. For example, the resonance from the Al13 polyhydroxyoxoaluminum cation must be multiplied by 13 whereas the resonance fro...

example 2

[0189]The remainder of the solution from which the aliquot was taken in Example 1 was continuously heated at 95° C. and stirred under reflux for a period of 24 hours. An aliquot was removed and subjected to testing by SEC chromatography and 27Al NMR spectroscopy.

[0190]As illustrated in FIG. 3, the SEC chromatogram shows, like FIG. 1, exclusively SEC-Peak 4 and SEC-Peak 5. No SEC-Peak 3 species is observed. No SEC-Peak 1 species or SEC-Peak 2 species is observed. The SEC-Peak 4 area comprised 98.2%, i.e. at least 90%, of the total area of Peaks 1, 2, 3, 4 and 5 in the SEC chromatogram. The SEC-Peak 5 area comprised 1.8%, i.e. less than 5%, of the total area of Peaks 1, 2, 3, 4 and 5 in the SEC chromatogram.

[0191]As illustrated in FIG. 4, the 27Al NMR spectrum shows a peak at approximately 70 ppm, representing the Al30 polyhydroxyoxoaluminum cation, and a peak at approximately 62.5 ppm, representing the Al13 polyhydroxyoxoaluminum cation. The peak ratios show, like FIG. 2, the Al30 po...

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Abstract

An antiperspirant active composition comprising an aluminum salt, the aluminum salt (i) having an aluminum to chloride molar ratio of 0.3:1 to 3:1; and (ii) exhibiting an 27Al NMR spectrum with a species distribution including at least 90% A130 polyhydroxyoxoaluminum cation as the predominant species detectable by 27Al NMR within the aluminum salt. The composition can optionally include zirconium. Also disclosed are a method of making an antiperspirant active composition and the use of a heating step at elevated temperature to convert Al13 polyhydroxyoxoaluminum cations in the species detectable by 27Al NMR within an aqueous aluminum salt solution into Al30 polyhydroxyoxoaluminum cations in the species detectable by 27Al NMR without increasing a SEC Peak 3 area in the SEC chromatogram of the aluminum salt.

Description

BACKGROUND[0001]The invention relates to antiperspirant active compositions comprising an aluminum salt and to methods of making an antiperspirant active composition.[0002]Antiperspirant salts, such as aluminum chlorohydrex (also called aluminum chlorohydrex polymeric salts and abbreviated here as “ACH”) and aluminum zirconium glycine salts (abbreviated here as “ZAG”, “ZAG complexes” or “AZG”), are known to contain a variety of polymeric and oligomeric species with molecular weights (MW) of 100 Da-500,000 Da. It has been clinically shown that, in general, the smaller the species, the higher the efficacy for reducing sweat.[0003]In an attempt to increase the quality and quantity of smaller aluminum and / or zirconium species, a number of efforts have focused on: (1) how to select the components of ACH and ZAG that affect the performance of these materials as antiperspirants; and (2) how to manipulate these components to obtain and / or maintain the presence of smaller types of these comp...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): A61K8/26A61Q15/00C01F7/57C01F7/78
CPCA61Q15/00A61K8/26C01P2002/86C01P2002/87A61K8/44C01F7/78C01F7/57A61K8/28A61K2800/80A61K2800/592
Inventor PAPPAS, IRAKLISPAN, LONG
Owner COLGATE PALMOLIVE CO
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